A combinatorial chemistry technique called parallel synthesis is used to create libraries of structurally related chemical compounds which are then screened to identify the most desirable varieties of these structurally related compounds. The chemical compounds that pass the screening phase are then reacted and tested to determine which of them are most suitable for manufacturing. This later reaction and testing stage, usually referred to as process optimization, requires precise control of the heat input to the reaction process and the ability to quickly absorb any heat generated by exothermic reactions which, by necessity, must be individualized for each chemical compound being tested. To obtain efficiency of scale, a number of chemical compounds must be reacted and tested at one time creating difficulties in individually controlling the heat input to and absorbing the heat output of each chemical compound.
Additionally, since a relatively large quantity of each chemical compound is required for the process optimization testing, which quantity is considered large at least when compared with the quantities of each compound utilized during parallel synthesis, the reaction vessels are relatively large thereby limiting the size of the array of reaction vessels that can be readily accommodated in a laboratory. To avoid reducing even further the number of reaction vessels that can be handled in a conveniently sized array, the size of the temperature control elements for each reaction vessel must be limited. However, the ability to control exothermic reactions in such relatively large reaction vessels is critical and requires rapid cooling capacity. Further, precise control of the temperature-time slope of the heat input to each reaction vessel is necessary. This requires close control of the heat input and output for each reaction vessel. Accordingly, it is required that the temperature control elements, although compact in size, have high output and efficiency, both in their heating and in their cooling capacities.
Recent technological advancements in the area of new compound discovery are accelerating the rate that new compounds are discovered. The recently developed techniques of combinatorial chemistry and high throughput screening are the driving force behind this increased rate in the discovery of new compounds. The importance of these techniques is reflected by the fact that these techniques are already being applied to new compound discovery efforts in a variety of different industries, including the pharmaceutical, chemical, petrochemical, materials, food, biotechnology, and cosmetic industries. Additionally, few technologies have been accepted into the R&D laboratory as readily in such a short period of time as combinatorial chemistry and high throughput synthesis.
This increased rate of new compound discovery is beginning to create an increased demand on the activities of the process development laboratories of the respective industries. The process development activities of process screening, process optimizing and process characterizing must increase to meet the increased level of effort required. Increasing the rate of these activities in the process development laboratory will require the implementation of automation in these labs. Some automation currently exists for supporting the activities of process screening and process characterizing.
This invention is directed to an apparatus for general organic synthesis which is suitable for process optimization in order to bridge the gap between process screening and manufacturing and process characterization in the process development laboratory.
The apparatus of this invention permits a number of simultaneous chemical reactions with each chemical reaction having a sufficient volume to permit mimicking of the physical conditions found in the manufacturing environment.
A feature of this invention is an apparatus for process optimization synthesis which allows for individual controls of reaction times and temperatures of each of a number of reaction vessels arranged in an array.
Another feature of this invention is an apparatus for process optimization synthesis which provides for refluxing inert environments, magnetic mixing and removal of samples of the reacted chemicals for analysis in real time.
Another feature of this invention is a reaction block having a compact temperature control mechanism.
Another feature of this invention is a reaction block which can control exothermic reactions of chemical compounds through high capacity thermoelectric cooling.
Another feature of this invention is a reaction block which can control endothermic reactions of chemical compounds through high capacity thermoelectric heating.
Another feature of this invention is a reaction block having temperature control mechanisms which permit the precise control of the temperature-time slope of the reaction of a chemical compound in a reaction vessel.
Another feature of this invention is a reaction block having a thermoelectric heater and cooler in which the thermoelectric elements are cascaded for increased heating and cooling capabilities.
Another feature of this invention is a heating and cooling arrangement for a reaction vessel which provides higher capacity refluxing than can be obtained with fluid cooling.
Other objects and advantages of this invention will be found in the following specification, claims and drawings.